Dimethyl Sulfate → 3-Methyl Flunitrazepam

HRID 1278482Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1278482
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[O:22])[CH:10]([CH3:23])[N:9]=1.[C:24](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[N:12]([CH3:24])[C:11](=[O:22])[CH:10]([CH3:23])[N:9]=1

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 20542078(+)-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazepin-2-one

Produkt 1

HCID 205623323-Methyl Flunitrazepam

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

95 g (0.30 M) of rac-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazepin-2-one are dissolved in 1 liter of absolute acetone and treated with 60 g of powdered potassium carbonate and 43 g of dimethyl sulphate. The mixture is stirred at room temperature for 4 hours and left to stand in a refrigerator for 48 hours. The mixture is then concentrated, treated with ice-water and extracted several times with methylene chloride. The organic solution is dried over sodium sulphate, filtered and concentrated. The residue is crystallised from ethyl acetate/petroleum ether, there being obtained rac-5-(o-fluorophenyl)-1,3-dihydro-1,3-dimethyl-7-nitro-2H-1,4-benzodiazepin-2-one which melts at 154°-156° C.

Aufarbeitung

  1. waitleft
  2. waitto stand in a refrigerator for 48 hours
  3. concentrationThe mixture is then concentrated
  4. additiontreated with ice-water
  5. extractionextracted several times with methylene chloride
  6. dry with materialThe organic solution is dried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue is crystallised from ethyl acetate/petroleum ether, there

Quellen und Nachweise

ORD-Eintrag
ord-5188d8103d524994950c48547c40c040
Quelldatensatz
uspto-grants-1981_07
Patentnummer
US04281188

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